UPLC同时测定五味子木脂素纯化物中15个化学成分的含量  

Simultaneous determination of fifteen components in purified lignans from Schisandrae Chinensis Fructus by UPLC

作　　者：张金朋 郭晓帆 杨园园 赵志远 李炳龙 刘媛媛 齐永秀 ZHANG Jin-peng;GUO Xiao-fan;YANG Yuan-yuan;ZHAO Zhi-yuan;LI Bing-long;LIU Yuan-yuan;QI Yong-xiu(School of Pharmaceutical Sciences,Shandong First Medical University&Shandong Academy of Medical Sciences,Taian 271016,China)

机构地区：[1]山东第一医科大学(山东省医学科学院)药学院,泰安271016

出　　处：《药物分析杂志》2022年第10期1697-1707,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：山东省医药卫生科技发展计划项目(202013030205);泰安市科技创新发展项目(2020NS166);大学生创新训练项目(202110439007和S202010439108)。

摘　　要：目的:建立采用UPLC同时测定五味子木脂素纯化物中五味子甲素、五味子乙素、五味子丙素、五味子醇甲、五味子醇乙、五味子酯甲、五味子酯乙、戈米辛D、当归酰戈米辛H、当归酰戈米辛Q、戈米辛G、戈米辛K、五味子酚、苯甲酰戈米辛H和戈米辛J共15个化学成分含量的方法。方法:采用Ultimate UHPLC XB-C_(18)色谱柱(100 mm×2.1 mm,1.8μm),以0.1%甲酸水(A)和0.1%甲酸乙腈(B)为流动相,梯度洗脱,流速0.3 mL·min^(-1),柱温为40℃,检测波长为267 nm,进样体积1μL。结果:3个批次中上述15个成分的含量范围为五味子甲素(4.02%~4.80%)、五味子乙素(4.85%~5.34%)、五味子丙素(0.15%~0.21%)、五味子醇甲(12.14%~12.64%)、五味子醇乙(2.72%~3.23%)、五味子酯甲(0.79%~0.87%)、五味子酯乙(2.65%~3.01%)、戈米辛D(0.53%~0.63%)、当归酰戈米辛H(2.33%~2.51%)、当归酰戈米辛Q(0.70%~0.81%)、戈米辛G(0.40%~0.45%)、戈米辛K(2.24%~3.07%)、五味子酚(0.94%~1.16%)、苯甲酰戈米辛H(0.27%~0.31%)、戈米辛J(0.71%~0.79%)。上述15个木脂素化学成分分离度良好且在线性范围内线性关系良好,平均回收率100.6%~103.1%,RSD为1.1%~4.0%。结论:该方法对五味子木脂素纯化物中15个化学成分同时进行含量测定,操作简单、准确且重复性好,可用于五味子的质量控制与评价及为后续药效学、药代动力学研究鉴定物质基础。Objective:To develop an UPLC method for simultaneous determination of deoxyschisandrin,schisandrin B,schisandrin C,schisandrol A,schisandrol B,schisantherin A,schisantherin B,gomisin D,angeloylgomisin H,angeloylgomisin Q,gomisin G,gomisin K,schisanhenol,benzoylgomisin H and gomisin J in the purified lignans of Schisandrae Chinensis Fructus.Methods:The components were separated on an Ultimate UHPLC XB-C_(18)column(100 mm×2.1 mm,1.8μm)with 0.1%formic acid aqueous solution(A)and 0.1%formic acid acetonitrile solution(B)as the mobile phase by gradient elution at a flow rate of 0.3 mL·min^(-1).The column tempera ture was set at 40℃,the detection wavelength was 267 nm,and the injection volume was 1μL.Results:The content ranges of deoxyschisandrin,schisandrin B,schisandrin C,schisandrol A,schisandrol B,schisantherin A,schisantherin B,gomisin D,angeloylgomisin H,angeloylgomisin Q,gomisin G,gomisin K,schisanhenol,benzoylgomisin H and gomisin J in 3 batches were 4.02%-4.80%,4.85%-5.34%,0.15%-0.21%,12.14%-12.64%,2.72%-3.23%,0.79%-0.87%,2.65%-3.01%,0.53%-0.63%,2.33%-2.51%,0.70%-0.81%,0.40%-0.45%,2.24%-3.07%,0.94%-1.16%,0.27%-0.31%and 0.71%-0.79%,respectively.The linear relationships of fifteen components were good in corresponding concentrations.The average recoveries of fifteen components were 100.6%-103.1%with the RSDs within 1.1%-4.0%.Conclusion:The method is rapid,accurate and suitable for simultaneous determination of 15 chemical components in the purified lignans.The method can provide reference for the quality control of Schisandrae Chinensis Fructus,and provide the pharmacodynamic material basis for the follow-up pharmacodynamics and pharmacokinetics studies.

关 键 词：五味子 木脂素纯化物 五味子甲素 五味子乙素 五味子丙素 五味子醇甲 五味子醇乙 五味子酯甲 五味子酯乙 戈米辛 当归酰戈米辛 五味子酚 苯甲酰戈米辛 含量测定 超高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]